CN1275153A - Method of coating luminescent material - Google Patents
Method of coating luminescent material Download PDFInfo
- Publication number
- CN1275153A CN1275153A CN99801332.3A CN99801332A CN1275153A CN 1275153 A CN1275153 A CN 1275153A CN 99801332 A CN99801332 A CN 99801332A CN 1275153 A CN1275153 A CN 1275153A
- Authority
- CN
- China
- Prior art keywords
- luminescent material
- luminescent
- discharge lamp
- aqeous suspension
- sequestering agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000000576 coating method Methods 0.000 title abstract description 16
- 239000011248 coating agent Substances 0.000 title abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical class OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000003352 sequestering agent Substances 0.000 claims description 6
- 229940048820 edetates Drugs 0.000 claims description 5
- 239000012456 homogeneous solution Substances 0.000 claims description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 229910016066 BaSi Inorganic materials 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 229910017639 MgSi Inorganic materials 0.000 claims description 3
- 229910004283 SiO 4 Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
- BYSUYBCCLCSGPR-UHFFFAOYSA-N 1h-pyrazol-5-yloxyboronic acid Chemical class OB(O)OC1=CC=NN1 BYSUYBCCLCSGPR-UHFFFAOYSA-N 0.000 claims description 2
- 229920000388 Polyphosphate Polymers 0.000 claims description 2
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical group CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 150000003983 crown ethers Chemical class 0.000 claims description 2
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 2
- 229940009662 edetate Drugs 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 150000002466 imines Chemical class 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- 239000001205 polyphosphate Substances 0.000 claims description 2
- 235000011176 polyphosphates Nutrition 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000002738 chelating agent Substances 0.000 abstract 1
- 230000005855 radiation Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000006862 quantum yield reaction Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
- C09K11/592—Chalcogenides
- C09K11/595—Chalcogenides with zinc or cadmium
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/666—Aluminates; Silicates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J61/00—Gas-discharge or vapour-discharge lamps
- H01J61/02—Details
- H01J61/38—Devices for influencing the colour or wavelength of the light
- H01J61/42—Devices for influencing the colour or wavelength of the light by transforming the wavelength of the light by luminescence
- H01J61/44—Devices characterised by the luminescent material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J61/00—Gas-discharge or vapour-discharge lamps
- H01J61/02—Details
- H01J61/38—Devices for influencing the colour or wavelength of the light
- H01J61/42—Devices for influencing the colour or wavelength of the light by transforming the wavelength of the light by luminescence
- H01J61/46—Devices characterised by the binder or other non-luminescent constituent of the luminescent material, e.g. for obtaining desired pouring or drying properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
- Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Vessels And Coating Films For Discharge Lamps (AREA)
- Formation Of Various Coating Films On Cathode Ray Tubes And Lamps (AREA)
Abstract
The invention relates to a method of coating a luminescent material with a layer of a metal oxide M2O3 wherein a metal M is chosen from the group formed by Y, AI and La. According to the invention, a watery solution of a complex of M and an organic chelating agent is added to a suspension of the luminescent material after which the luminescent material is separated dried and fired.
Description
The present invention relates to use M
2O
3Metal oxide layer applies the method for luminescent material, and described metal M is selected from Y, Al and La, wherein by being deposited on this luminescent material from the compound of aqueous solution precipitation from homogeneous solution mode with M.
The invention still further relates to through this method and obtain luminescent material, and relate to the discharge lamp that luminescent screen is housed, this luminescent screen contains this luminescent material.
WO 96/05265 discloses as first section described method.Show advantages of higher stability in the water paste that coated luminescent material uses in the light fixture production process, and a kind of light output continuity of improvement.One of shortcoming of prior art is that many luminescent materials (material that the silicate host lattice for example, is arranged) are easy to hydrolysis when precipitation from homogeneous solution takes place low pH value.In addition, also through finding, in water unhydrolyzed other luminescent material for example the optical property of reflectivity and quantum yield be subjected to the injury of low pH value.
The purpose of this invention is to provide by precipitation from homogeneous solution from the aqueous solution, make the method for metal oxide-coated luminescent material, wherein from having prevented luminescent material hydrolysis and its optical performance degradation to a great extent.
According to the present invention, method described in first section is suitable for this purpose, it is characterized in that, in turn, preparation luminescent material aqeous suspension, in this aqeous suspension, add the aqueous solution of the title complex that contains M and organic sequestering agent, from this aqeous suspension, isolate this luminescent material and carry out drying and heating.
Have been found that organic sequestering agent has stoped M (OH)
3Precipitation.Consequently, can under higher pH value precipitation from homogeneous solution take place.Therefore, strongly inhibited the hydrolysis and the deterioration of luminescent material.
As organic sequestering agent, obtained good result with quadrol, three pyrazolyl borates, diglyme, phenylformic acid, crown ether, polyphosphate and the three hot imines of ring (triazacyclononane).Especially obtained better result with edetate.
The pH value scope of aqeous suspension be 8～10 and the pH value of aqueous solution scope be under 6.5～7.5 the situation, also to have obtained good result.The meticulous granular coating that relies on the luminescent material that the inventive method obtained is generally by the spherical Me of diameter less than 30 nanometers
2O
3The thin layer of nanoparticle is formed.This coating and the coating that relies on CVD to apply can be made a distinction with scanning electronic microscope or tem study.The performance of this coating also characteristic by the observable phosphor of naked eyes (phosphor) obtains embodying, and for example compares with the coating that the CVD method applies, because the surface is more cleaned the higher enhanced light that causes slightly of scattering is exported.
Method of the present invention is particularly suited for applying the luminescent material with silicate host lattice (silicate host lattice), because these luminescent materials are very easy to hydrolysis in the aqueous solution of low pH value.Particularly verified, this method is very suitable for using La
2O
3Coated with plumbous activatory BaSi
2O
5, with the aluminium activatory (Ba, Sr)
2MgSi
2O
7With with manganese-activated Zn
2SiO
4
Find, be highly suitable for the luminescent screen of the luminescent screen, particularly low-pressure mercury discharge lamp of discharge lamp according to the luminescent material of the inventive method coating.
To illustrate the present invention by describing 3 embodiments now.
In first embodiment, use La
2O
3Apply with plumbous activatory BaSi
2O
5(BSP).To 250 milligrams of La
2O
3Be dissolved in and add 125 milligrams of edetates (EDTA) in 50 milliliters of solution that softening water became.Add Ba (OH)
2The pH value of this solution is adjusted to about 7.
With Ba (OH)
2Adding in another softening water of 50 milliliters, is about 9.5 until the pH value.After this, in this solution, add 10 gram BSP.LA (EDTA) drips of solution is added in the BSP suspension.After in BSP suspension, adding whole LA (EDTA) solution, add Ba (OH) once more
2The pH value of this suspension is adjusted to about 9.5.Stir this suspension then 2 hours, and follow the BSP that filtering separation applies.At last, wash this phosphor, fired 2 hours 80 ℃ of following dryings and in 900 ℃ with alkaline water.Basically identical (the λ max=350nm of the emmission spectrum of the BSP that applies and uncoated BSP; FVMM=38nm).The reflection coefficient of 254 nanometers and 350 nm radiations also almost consistent (uncoated BSP is respectively 20% and 96%, and the BSP of coating is respectively 19% and 95%).Yet surprisingly, the quantum yield of 254 nm radiations of the BSP that discovery applies is than uncoated BSP high by 6% (being respectively 94% and 88%).
In second embodiment, use La
2O
3Apply with plumbous activatory (Ba, Sr)
2MgSi
2O
7(SMS).Used coating method is consistent with the coating method of described BSP before this, but with Sr (OH)
2Replace Ba (OH)
2Apply and the emmission spectrum basically identical (λ max=360nm:FVMM=60nm) of uncoated SMS.Find to apply and the quantum yield of 254 nm radiations of uncoated SMS is 75%.254 nanometers of uncoated SMS and the reflection coefficient of 350 nm radiations are respectively 8% and 96%, and the SMS of coating is respectively 10% and 95%.
In the 3rd embodiment, use La
2O
3Apply and use manganese-activated Zn
2SiO
4(ZSM).Used coating method is consistent with the coating method of described BSP before this, but replaces Ba (OH) with NaOH
2Apply and emmission spectrum basically identical (the λ max=520nm of uncoated ZSM; FVMM=41nm).Find to apply and the quantum yield of uncoated ZSM is respectively 79% and 80%.The reflection coefficient of 254 nm radiations of the uncoated ZS and the ZSM of coating is respectively 94% and 93%.
Claims (13)
1. use M for one kind
2O
3Metal oxide layer applies the method for luminescent material, wherein metal M is selected from Y, Al and La, wherein the compound of M is deposited on this luminescent material by precipitation from homogeneous solution, it is characterized in that, in turn, preparation luminescent material aqeous suspension, interpolation contains the aqueous solution of the title complex of M and organic sequestering agent in this aqeous suspension, isolates this luminescent material and carry out drying and heating from this aqeous suspension.
2. according to the process of claim 1 wherein that this organic sequestering agent is selected from quadrol, three pyrazolyl borates, diglyme, phenylformic acid, crown ether, polyphosphate and three hot imines of ring and edetates.
3. the method described in claim 2, wherein organic sequestering agent is an edetate.
4. the method described in claim 1,2 or 3, wherein the pH value of this aqeous suspension is in 8～10 scope.
5. one or multinomial described method in the claim as described above, wherein this pH value of aqueous solution is in 6.5～7.5 scope.
6. use M
2O
3The luminescent material that metal oxide layer applies, wherein metal M is selected from Y, Al and La, and this material is according to one or multinomial described method acquisition in the aforementioned claim.
7. according to the luminescent material of claim 6, contain the silicate host lattice.
8. according to the luminescent material of claim 7, contain useful plumbous activatory BaSi
2O
5
9. according to the luminescent material of claim 7, contain useful plumbous activatory (Ba, Sr)
2MgSi
2O
7
10. according to the luminescent material of claim 7, contain useful manganese-activated Zn
2SiO
4
11. according to claim 6,7,8,9 or 10 luminescent material, wherein M is La.
12. the discharge lamp of luminescent screen is housed, and this luminescent screen comprises according to one of claim 6～11 or multinomial luminescent material.
13. according to the discharge lamp of claim 12, wherein this discharge lamp is a low-pressure mercury discharge lamp.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP98202848 | 1998-08-25 | ||
| EP98202848.2 | 1998-08-25 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1275153A true CN1275153A (en) | 2000-11-29 |
| CN1218013C CN1218013C (en) | 2005-09-07 |
Family
ID=8234061
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99801332.3A Expired - Fee Related CN1218013C (en) | 1998-08-25 | 1999-08-23 | Method of coating luminescent material |
Country Status (6)
| Country | Link |
|---|---|
| US (2) | US6472811B1 (en) |
| EP (1) | EP1047750B1 (en) |
| JP (1) | JP2002523551A (en) |
| CN (1) | CN1218013C (en) |
| DE (1) | DE69924601T2 (en) |
| WO (1) | WO2000011104A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295297C (en) * | 2005-02-25 | 2007-01-17 | 东南大学 | Alumina coated fluorescent powder and its coating method |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19901538A1 (en) * | 1999-01-16 | 2000-07-27 | Philips Corp Intellectual Pty | Screen with fluorescent preparation containing metal oxide |
| FR2801299B1 (en) * | 1999-11-23 | 2002-06-07 | Rhodia Terres Rares | AQUEOUS COLLOIDAL DISPERSION BASED ON AT LEAST ONE COMPOUND OF A LANTHANIDE AND A COMPLEXANT, METHOD OF PREPARATION AND USE |
| EP1322722A1 (en) * | 2000-06-22 | 2003-07-02 | S.L.E. (Australia) Pty Ltd | Phosphorescent pigments |
| AU2001267136B2 (en) * | 2000-06-22 | 2006-01-05 | Nite-Glo Innovations Pty Ltd | Phosphorescent pigments |
| US6761971B2 (en) * | 2001-09-26 | 2004-07-13 | Osram Sylvania Inc. | Protective spinel coating for aluminate phosphors |
| DE102004063217A1 (en) * | 2004-12-29 | 2006-07-13 | Giesecke & Devrient Gmbh | Security feature for value documents |
| EP2593527B1 (en) * | 2010-07-13 | 2014-04-02 | Koninklijke Philips N.V. | Uv-a or uv-b-emitting discharge lamp |
| CN103275708B (en) * | 2013-02-28 | 2016-06-15 | 福建省长汀金龙稀土有限公司 | A kind of surface-coating method of lamp BAM fluorescent material |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL152291B (en) * | 1967-03-01 | 1977-02-15 | Philips Nv | MERCURY VAPOR DISCHARGE LAMP WITH A LUMINESCENT MATERIAL. |
| LU71476A1 (en) * | 1974-04-22 | 1975-06-17 | ||
| US4522958A (en) * | 1983-09-06 | 1985-06-11 | Ppg Industries, Inc. | High-solids coating composition for improved rheology control containing chemically modified inorganic microparticles |
| DE3578599D1 (en) * | 1984-05-07 | 1990-08-16 | Gte Laboratories Inc | METHOD FOR COATING PHOSPHORIC PARTICLES, PHOSPHORIC PARTICLES, FLUORESCENT LAMP AND METHOD FOR PRODUCING THE SAME. |
| EP0476207A3 (en) * | 1990-09-17 | 1992-04-08 | Gte Products Corporation | Improved lead-activated barium silicate phosphor and method of making same |
| US5382452A (en) * | 1992-12-18 | 1995-01-17 | E. I. Du Pont De Nemours And Company | Luminescent materials prepared by coating luminescent compositions onto substrate particles |
| EP0638625B1 (en) * | 1993-07-30 | 2002-09-11 | Toshiba Lighting & Technology Corporation | Luminescent material for a mercury discharge lamp |
| DE69526423T2 (en) * | 1994-08-08 | 2002-12-05 | Koninkl Philips Electronics Nv | METHOD FOR COATING A LUMINESCENT MATERIAL |
| KR19980046311A (en) * | 1996-12-12 | 1998-09-15 | 손욱 | Fluorescent projector |
| US6001477A (en) * | 1997-01-03 | 1999-12-14 | Osram Sylvania Inc. | Phosphor powder for coating lamp envelopes and method for preparation |
| DE19727607C2 (en) * | 1997-06-28 | 2000-11-23 | Philips Corp Intellectual Pty | Plasma screen with a UV phosphor preparation and UV phosphor preparation |
-
1999
- 1999-08-23 WO PCT/EP1999/006162 patent/WO2000011104A1/en active IP Right Grant
- 1999-08-23 EP EP99944474A patent/EP1047750B1/en not_active Expired - Lifetime
- 1999-08-23 JP JP2000566363A patent/JP2002523551A/en active Pending
- 1999-08-23 DE DE69924601T patent/DE69924601T2/en not_active Expired - Lifetime
- 1999-08-23 CN CN99801332.3A patent/CN1218013C/en not_active Expired - Fee Related
- 1999-08-25 US US09/383,291 patent/US6472811B1/en not_active Expired - Fee Related
-
2002
- 2002-05-10 US US10/143,436 patent/US6833160B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295297C (en) * | 2005-02-25 | 2007-01-17 | 东南大学 | Alumina coated fluorescent powder and its coating method |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2000011104A1 (en) | 2000-03-02 |
| DE69924601T2 (en) | 2006-03-02 |
| CN1218013C (en) | 2005-09-07 |
| JP2002523551A (en) | 2002-07-30 |
| US6833160B2 (en) | 2004-12-21 |
| US20020127329A1 (en) | 2002-09-12 |
| DE69924601D1 (en) | 2005-05-12 |
| EP1047750B1 (en) | 2005-04-06 |
| US6472811B1 (en) | 2002-10-29 |
| EP1047750A1 (en) | 2000-11-02 |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20050907 Termination date: 20120823 |